CN106083062B - A kind of ceramic material and preparation method thereof for superhigh temperature impression instrument pressure head - Google Patents
A kind of ceramic material and preparation method thereof for superhigh temperature impression instrument pressure head Download PDFInfo
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- CN106083062B CN106083062B CN201610403258.5A CN201610403258A CN106083062B CN 106083062 B CN106083062 B CN 106083062B CN 201610403258 A CN201610403258 A CN 201610403258A CN 106083062 B CN106083062 B CN 106083062B
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
- C04B35/58064—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
- C04B35/58078—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on zirconium or hafnium borides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3826—Silicon carbides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3886—Refractory metal nitrides, e.g. vanadium nitride, tungsten nitride
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Abstract
The present invention relates to a kind of ceramic materials and preparation method thereof for superhigh temperature impression instrument pressure head, belong to superhigh temperature structural material field.The mass component content of ceramic material of the present invention is：Zirconium boride 40-60%, zirconium nitride 5-15%, titanium nitride 5-15%, vanadium nitride 5-15%, silicon carbide 15-25%.Preparation method is：After ball milling and drying by dispensing, it is fitted into molding die, in an inert atmosphere Isothermal sinter, obtains ceramic material.The ceramic material of the present invention still has higher mechanical behavior under high temperature and good inoxidizability at higher temperature (1000 DEG C of >), and the preparation process of the ceramic material is simple；By the Machining of Ceramics of the present invention at impression instrument ceramics pressure head, it is applicable to the impression detection of ultra-high temperature section.
Description
Technical field
The present invention relates to a kind of ceramic materials and preparation method thereof for superhigh temperature impression instrument pressure head, belong to superhigh temperature
Structural material field.
Background technology
Aero-engine is known as " heart " of aircraft, is an important factor for restricting Development of China's Aviation Industry.Improve boat
The thrust-weight ratio of empty engine is the target that aircraft designers constantly pursue.And it is to improve aeroplane engine to improve turbine inlet temperature (TIT)
The important channel of machine thrust-weight ratio.Monocrystalline high temperature metallic material, cooling air membrane technology and advanced thermal barrier coating are referred to as improving turbine
Three big key technologies of inlet temperature.Particularly, advanced thermal barrier coating is considered as improving engine turbine inlet temperature most to cut
Real feasible method.Thermal barrier coating is coated in the surface of aero-engine metal parts, protects metal parts from high temperature gas flow
Erosion.However, damage inactivation of thermal barrier coating during military service restricts the application and development of thermal barrier coating.Therefore, it opens
The research of exhibition thermal barrier coating damage inactivation is of great significance to the application and development that promote thermal barrier coating.The destruction of thermal barrier coating is lost
Effect is the complicated dynamic process under Re-power-oxygen collective effect, understands that its Basic Mechanism and rule are needed to thermal barrier coating service mistake
Mechanical property in journey is tested and is characterized.Thermal barrier coating is usually on active service under high temperature environment, and mechanical property can take
It changes during labour, therefore, it is necessary to test and characterize the mechanical property of thermal barrier coating under hot environment.
Thermal barrier coating (is such as stretched, is compressed, bending as a kind of typical multilayered structure, traditional macro-test method
And shearing etc.) there is limitations in terms of testing its mechanical property.Indentation is as a kind of widely applied local mechanical
Test method has big advantage in terms of testing stratiform material mechanical performance.Indentation has been used for thermal barrier coating room temperature
The test of mechanical property, but it is all very rare both at home and abroad about mechanical behavior under high temperature test, it can be used for high temperature this is because lacking
The impression instrument of environmental testing.Currently, the maximum operation (service) temperature of external high temperature impression instrument is 950 DEG C, it is not enough to covering thermal boundary
The service temperature (- 1250 DEG C of room temperature) of coating；And the country yet there are no relevant report.Therefore, research and development are suitable under Service Environment
The superhigh temperature impression instrument of thermal barrier coating Mechanics Performance Testing is for promoting the development of the aircraft industry and Defence business in China to have
It is significant.
One of great difficult problem in superhigh temperature impression instrument R&D process is high temperature pressure head technology, including high-temperature high-pressure head material
Type selecting and prepare processing, this is also to restrict an important factor for high temperature impression instrument test temperature is further promoted.According to
The basic principle of impression test, high temperature pressure head should have higher hardness and intensity, preferable chemical stabilization under high temperature environment
Property and oxidation resistance.Existing high temperature impression instrument mostly uses diamond and cube nitrogen greatly in lower temperature section (500 DEG C of <)
Change zirconium pressure head, sapphire and tungsten carbide pressure head are mostly used greatly in higher temperature section (500-950 DEG C).And above-mentioned pressure head is due to oxidation
The problems such as decomposition, strength retrogression, higher temperature can not be applied to.Therefore, pressure head technology pair of the research and development suitable for higher temperature
It is particularly significant in the power of test of elevating ultrahigh temperature and pressure trace instrument.
Invention content
The purpose of the present invention is to solve the pressures that the pressure head material of conventional indentation instrument can not be suitable for ultra-high temperature section
Trace detects, and provides a kind of ceramic material and preparation method thereof for superhigh temperature impression instrument pressure head, which compares
There are the non-oxide ceramics of more preferable mechanical property, more preferable chemical stability and oxidation resistance in oxide ceramic material system
Material system (zirconium boride (ZrB2)-zirconium nitride (ZrN)-titanium nitride (TiN)-vanadium nitride (VN)-silicon carbide (SiC)), utilize heat
Pressure is sintered, the method for electric machining is prepared into ceramic pressure head.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of ceramic material for superhigh temperature impression instrument pressure head of the present invention, the quality of each component in the ceramic material
Percentage is as follows：
Zirconium boride 40-60%,
Zirconium nitride 5-15%,
Titanium nitride 5-15%,
Vanadium nitride 5-15%,
Silicon carbide 15-25%,
Wherein, the grain size of zirconium boride is 1.0-2.0 μm, and the grain size of zirconium nitride is 0.5-2.5 μm, and the grain size of titanium nitride is
1.0-2.0 μm, the grain size of vanadium nitride is 0.8-1.6 μm, and the grain size of silicon carbide is 0.5-2 μm.
A kind of ceramic material preparation method for superhigh temperature impression instrument pressure head of the present invention, preparation method include such as
Lower step：
1) dispensing is carried out according to following mass percents：Zirconium boride 40-60%, zirconium nitride 5-15%, titanium nitride 5-15%,
Vanadium nitride 5-15%, silicon carbide 15-25%；Wherein, the grain size of zirconium boride is 1.0-2.0 μm, and the grain size of zirconium nitride is 0.5-2.5
μm, the grain size of titanium nitride is 1.0-2.0 μm, and the grain size of vanadium nitride is 0.8-1.6 μm, and the grain size of silicon carbide is 0.5-2 μm；
2) after mixing the dispensing that step 1) obtains with solvent, ball milling mixing is carried out in planetary ball mill；
3) it by the mixture after ball milling under 80-95 DEG C of temperature, stirring condition, dries 1-3 hours；
4) mixed powder after step 3) drying is crossed into 50-80 mesh sieve, the mixed powder after sieving is packed into molding die
In；
5) it is 10 in vacuum degree by the molding die equipped with mixed powder-3-10-2Under conditions of Mpa, with 10-25 degrees/min
Heating rate be heated to 1800-2000 DEG C after, be filled with inert gas and be forced into 10-40Mpa, it is small to carry out Isothermal sinter 0.5-2
When；
6) 60 DEG C are cooled the temperature to hereinafter, obtaining ceramic material with 10-25 degrees/min of cooling rate.
Solvent described in step 2) is alcohol, and the abrading-ball in ball grinder uses silicon carbide ceramics ball, wherein Ceramic Balls：Match
Material：The mass ratio of alcohol is 1：(1~1.5)：(2~4)；The speed of service of planetary ball mill is 180-240 revs/min, ball milling
Time is 8-12 hours.
Drying described in step 3) is to carry out heating water bath in a rotary evaporator, and rotary evaporator rotating speed is 20-50
Rev/min.
The above-mentioned ceramic material that obtains can be processed into superhigh temperature impression instrument pressure head by electric processing method.
Advantageous effect
The ceramic material of the present invention still has higher mechanical behavior under high temperature and good at higher temperature (1000 DEG C of >)
Inoxidizability, and the preparation process of the ceramic material is simple；By the Machining of Ceramics of the present invention at impression instrument ceramics
Pressure head is applicable to the impression detection of ultra-high temperature section.
Description of the drawings
Fig. 1 is the temperature-strength test data for the ceramic pressure head that embodiment obtains.
Specific implementation mode
The content of patent of the present invention is described further by the following examples：
Embodiment
A kind of preparation method for superhigh temperature impression instrument pressure head, specific preparation process are as follows：
1) dispensing is carried out according to the component formula of table 1 and the grain size being respectively formulated；
ZrB in 1 specific embodiment of table2The raw material tables of data of-ZrN-TiN-VN-SiC composite ceramics pressure heads
2) it after mixing the dispensing that step 1) obtains with 200g alcohol, is put into the ball grinder equipped with silicon carbide ceramics ball；
3) ball grinder equipped with dispensing is placed on progress ball milling mixing, the speed of service of planetary ball mill in planetary ball mill
It it is 240 revs/min, Ball-milling Time is 10 hours；
4) mixture after step 3) ball milling is dried in a rotary evaporator, wherein bath temperature is 90 DEG C, rotation
Bottle rotating speed is 40 revs/min, and drying time is 3 hours, and the mixed powder after drying crosses 60 mesh sieve, and the mixed powder after having screened is packed into
In molding die；
5) it is 10 in vacuum degree by the molding die equipped with mixed powder-3In sintering furnace under the conditions of MPa, with 20 degrees/min
Heating rate be heated to 1950 DEG C after, be filled with nitrogen and be forced into 30MPa, in 1950 DEG C of Isothermal sinters 1 hour；
6) fire door is opened after the temperature in sintering furnace being down to 60 DEG C with 20 DEG C/min of cooling rate, takes out ceramics
Material.
7) step 6) is obtained into ceramic material and impression instrument pressure head is processed by electric processing method.
The impression instrument pressure head that embodiment is obtained carries out high temperature three-point bending strength test, obtains temperature-intensity data
As shown in Figure 1.From fig. 1, it can be seen that using Machining of Ceramics of the present invention at impression instrument pressure head, intensity with temperature liter
Height first increases to be reduced afterwards, and higher numerical value is still remain at 1400 DEG C.
Claims (4)
1. a kind of ceramic material preparation method for superhigh temperature impression instrument pressure head, it is characterized in that：The preparation method includes such as
Lower step：
1) dispensing is carried out according to following mass percents：Zirconium boride 40-60%, zirconium nitride 5-15%, titanium nitride 5-15%, nitridation
Vanadium 5-15%, silicon carbide 15-25%；Wherein, the grain size of zirconium boride is 1.0-2.0 μm, and the grain size of zirconium nitride is 0.5-2.5 μm,
The grain size of titanium nitride is 1.0-2.0 μm, and the grain size of vanadium nitride is 0.8-1.6 μm, and the grain size of silicon carbide is 0.5-2 μm；
2) after mixing the dispensing that step 1) obtains with solvent, ball milling mixing is carried out in planetary ball mill；
3) it by the mixture after ball milling under 80-95 DEG C of temperature, stirring condition, dries 1-3 hours；
4) mixed powder after step 3) drying is crossed into 50-80 mesh sieve, the mixed powder after sieving is fitted into molding die；
5) it is 10 in vacuum degree by the molding die equipped with mixed powder-3-10-2Under conditions of MPa, with 10-25 degrees celsius/minutes
After heating rate is heated to 1800-2000 DEG C, it is filled with inert gas and is forced into 10-40MPa, carry out Isothermal sinter 0.5-2 hours；
6) 60 DEG C are cooled the temperature to hereinafter, obtaining ceramic material with the cooling rate of 10-25 degrees celsius/minutes.
2. a kind of ceramic material preparation method for superhigh temperature impression instrument pressure head as described in claim 1, it is characterized in that：
Solvent described in step 2) is alcohol, and the abrading-ball in ball grinder uses silicon carbide ceramics ball, wherein Ceramic Balls：Dispensing：
The volume ratio of alcohol is 1：(1~1.5)：(2~4)；The speed of service of planetary ball mill is 180-240 revs/min, Ball-milling Time
It is 8-12 hours.
3. a kind of ceramic material preparation method for superhigh temperature impression instrument pressure head as described in claim 1, it is characterized in that：
Drying described in step 3) is to carry out heating water bath in a rotary evaporator, rotary evaporator rotating speed be 20-50 turn/
Point.
4. a kind of superhigh temperature impression instrument pressure head, it is characterized in that：The pressure head is the ceramics prepared using claim 1 the method
Material is prepared by electric processing method.
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| CN201610403258.5A CN106083062B (en) | 2016-06-08 | 2016-06-08 | A kind of ceramic material and preparation method thereof for superhigh temperature impression instrument pressure head |
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| CN103626496B (en) * | 2013-12-05 | 2015-04-08 | 燕山大学 | Non-stoichiometric ratio TiC, AlN and TiN composite material |
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